CN110330814B - Grinding method of high-quality synthetic mica - Google Patents

Grinding method of high-quality synthetic mica Download PDF

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CN110330814B
CN110330814B CN201910680295.4A CN201910680295A CN110330814B CN 110330814 B CN110330814 B CN 110330814B CN 201910680295 A CN201910680295 A CN 201910680295A CN 110330814 B CN110330814 B CN 110330814B
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mica
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CN110330814A (en
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余海莹
朱秋莲
余淳秋
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Shantou Zhen Zhen Pearlescent Pigment Co ltd
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0015Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
    • C09C1/0021Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a core coated with only one layer having a high or low refractive index
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    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/40Compounds of aluminium
    • C09C1/405Compounds of aluminium containing combined silica, e.g. mica
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    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/041Grinding
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    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06Treatment with inorganic compounds
    • C09C3/063Coating
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    • C01P2004/60Particles characterised by their size
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    • C01P2006/00Physical properties of inorganic compounds
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    • C01P2006/00Physical properties of inorganic compounds
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    • C01P2006/60Optical properties, e.g. expressed in CIELAB-values
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    • C01P2006/60Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/66Hue (H*)

Abstract

The invention discloses a grinding method of high-quality synthetic mica, which comprises the following steps: a. crushing: crushing mica into 200-2000 mu m mica sheets by ultrahigh pressure hydraulic power; b. separation: putting the mica slices into a centrifugal separator for solid-liquid separation, and spin-drying water; c. grinding: selecting grinding equipment, adding grinding media or grinding aids, adding mica flakes, controlling moisture, grinding for 3-8 hours to form mica powder, pulping, and discharging; d. and (3) settling: and (4) pulping the ground mica powder, and separating the finished mica powder products of all the particle size sections by a hydraulic sedimentation method. Has the advantages that: according to the invention, after the crushed mica is crushed by ultrahigh pressure water power, the crushed mica is ground into slurry by a stirring mill and a mixed grinding medium and grinding aid, and then the finished mica powder of each particle size section is obtained by a hydraulic settlement method, so that the mica is not damaged and has no dust escaping in the grinding process, and the method has the advantages of less regrinding amount, high quality, energy conservation and environmental protection.

Description

Grinding method of high-quality synthetic mica
Technical Field
The invention relates to the technical field of mica powder production, in particular to a grinding method of high-quality synthetic mica.
Background
The pearlescent pigment is used as a novel decorative pigment and widely applied to the fields of paint, plastic, rubber, printing ink, leather, paper, ceramics, cosmetics, printing and dyeing and the like, and the artificially synthesized fluorophlogopite serving as a base material gradually replaces natural mica sheets with less impurities, good whiteness, good brightness and high chemical stability and becomes an important material for producing the mica titanium pearlescent pigment.
The grinding mode of the artificially synthesized mica powder is divided into a wet method and a dry method. The production of pearlescent pigment requires wet grinding of mica powder, and the wet ground mica has smooth surface, large diameter-thickness ratio and pure texture, and is beneficial to coating of metal oxide.
At present, the grinding of the artificially synthesized mica powder applied to the pearlescent pigment is mainly carried out by a wheel mill, and the principle is that small mica sheets, a grinding aid and a dispersing agent are added into a wheel milling groove which takes water as a grinding medium, and under the heavy pressure of a wheel mill, mica is peeled from a cleavage plane to form mica fragments which are separated from each other. However, the wheel milling has the following disadvantages:
1. the milling difficulty is large, and the cost is high: the synthetic mica has higher hardness than natural mica and is difficult to be ground, the ground material return sheets are more, the fine powder is more, the grinding needs to be repeated for many times, the efficiency is low, and the waste is large;
2. the ground large-piece has more proportion, the powder amount with the diameter of less than 100 mu m is too small, and the powder is not suitable for production requirements;
3. the diameter-thickness ratio difference is as follows: the color saturation and brightness of the coated pearly luster are influenced, and the yield is low;
to solve the above problems, a method of grinding high-quality synthetic mica has been proposed.
Disclosure of Invention
The present invention is directed to a method for grinding high-quality synthetic mica to solve the problems of the background art.
In order to achieve the purpose, the invention adopts the following technical scheme: a grinding method of high-quality synthetic mica comprises the following steps:
a. crushing: crushing mica into 200-2000 mu m mica sheets by ultrahigh pressure hydraulic power;
b. separation: putting the mica slices into a centrifugal separator for solid-liquid separation, and spin-drying water;
c. grinding: selecting grinding equipment, adding grinding media or grinding aids, adding mica flakes, controlling moisture, grinding for 3-8 hours to form mica powder, pulping, and discharging;
d. and (3) settling: pulping the ground mica powder, and separating the finished mica powder products of all particle size sections by a hydraulic sedimentation method;
the water pressure of the ultrahigh-pressure water is 6-12 Mpa;
the grinding aid is sodium hexametaphosphate accounting for 0.01-0.05% of the mass of the mica, sodium carbonate accounting for 0.01-0.05% of the mass of the mica and sodium hydroxide accounting for 0.01-0.03% of the mass of the mica;
the grinding medium is zirconium beads/column with the specification of 10x10mm, 7.5x7.5mm and 5x5 mm;
the grinding equipment is a stirring mill, and the rotating speed of the stirring mill is 50-120;
the grinding control water content is 25% -40%, and the water content is measured by a water content measuring instrument;
the solid-liquid ratio of the classification by the hydraulic sedimentation method is 10-15 percent;
the hydraulic sedimentation method is a gravity sedimentation method, an ascending water flow method or a centrifugal sedimentation method.
Compared with the prior art, the grinding method of the high-quality synthetic mica has the advantages that:
1. crushing the artificially synthesized fluorophlogopite powder by 6-12Mpa of ultrahigh pressure water to obtain smaller mica flakes, which is more convenient for subsequent grinding;
2. the grinding medium in the stirring mill is just better applied to the fine grinding of mica, so that the mica can be well delaminated by the friction force of the medium without damaging the surface of the mica;
3. obtaining finished mica powder products of all particle size sections of mica pulping by a hydraulic sedimentation method;
in conclusion, after mica particles are crushed by ultrahigh pressure water power, the mica particles are ground into slurry by a stirring mill and a mixed grinding medium and grinding aid, and then mica powder finished products of all particle size sections are obtained by a water power sedimentation method, so that mica is free of damage and dust escape in the grinding process, and the mica powder grinding method has the advantages of less regrinding amount, high quality, energy conservation and environmental protection.
Detailed Description
The following examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Example (b):
a grinding method of high-quality synthetic mica comprises the following steps:
a. crushing: crushing mica into 200-2000 mu m mica sheets by ultrahigh pressure hydraulic power; the water pressure of the ultrahigh pressure water is 6-12 Mpa.
b. Separation: putting the mica slices into a centrifugal separator for solid-liquid separation, and spin-drying water;
c. grinding: selecting grinding equipment, adding grinding media or grinding aids, adding mica flakes, controlling moisture, grinding for 3-8 hours to form mica powder, pulping, and discharging; the grinding equipment is a stirring mill, the rotation speed of the stirring mill is 50-120, the grinding medium is zirconium beads/columns with the specifications of 10x10mm, 7.5x7.5mm and 5x5mm, the grinding aids are sodium hexametaphosphate accounting for 0.01-0.05% of the mass of the mica, sodium carbonate accounting for 0.01-0.05% of the mass of the mica and sodium hydroxide accounting for 0.01-0.03% of the mass of the mica, the grinding control moisture is 25-40%, and the grinding control moisture is measured by a moisture tester.
d. And (3) settling: and (3) pulping the ground mica powder, and separating the mica powder finished products of all the particle size sections by a hydraulic sedimentation method, wherein the solid-liquid ratio of classification by the hydraulic sedimentation method is 10-15%, and the hydraulic sedimentation method is a gravity sedimentation method, an ascending water flow method or a centrifugal sedimentation method.
The gravity settling method is that the particles and fluid are caused to move relatively to settle under the action of gravitational field, and the particles are concentrated in one direction under the action of gravitational field, or sink to the bottom of the container or float to the upper layer of the medium as long as the density of the particles and the medium is different.
An ascending water flow method: the typical apparatus of the ascending water flow method is a continuous decanter, and the basic principle is that the same ascending water quantity is utilized to generate different ascending water velocities in classifying pipes with different diameters, and ore particles with different particle sizes are divided into a plurality of particle sizes according to different settling velocities.
Centrifugal sedimentation method: the device used in the centrifugal sedimentation method is a series cyclone classifier, also called a cyclone water analyzer, and the basic principle is that the classification process is carried out in a centrifugal force field, and substances are thrown out at different heights according to different centrifugal forces to which the substances with different specific gravities are subjected.
Crushing the artificially synthesized fluorophlogopite into 200-2000 mu m mica slices by hydraulic power of 0.8Mpa, collecting and drying the excessive water. Connecting a power supply of a stirring mill, starting a motor, adjusting stirring for 30-65 revolutions, adding 300 kilograms of grinding medium zirconium columns or zirconium beads, slowly adding 300 kilograms of mica fine pieces into dry pieces, adding 100 grams of grinding aid sodium hexametaphosphate, 100 grams of sodium carbonate and 50 grams of sodium hydroxide, controlling grinding moisture to be 30-40%, adjusting the rotating speed of the mill to be 50-120 revolutions, finishing grinding after 5 hours, unloading and grading, calculating the yield of each particle size section, enabling the medium to do irregular motion through high-speed rotation of a main shaft with a stirring rod, generating friction, collision, extrusion and shearing force, enabling synthetic mica powder with high hardness and difficult to be ground into fine-grained slices suitable for producing pearlescent pigment, enabling a master slice as a layered mineral which is a mineral difficult to be ground, enabling the grinding acting force of the mineral to be the best effect of the friction force, and grinding medium in the stirring mill, the mica fine grinding method has the advantages that the friction force is better applied to fine grinding of the mica, the mica is well stripped in a layered mode through the friction force of the medium, the surface of the mica is not damaged, meanwhile, no dust escapes, and the mica fine grinding method has the advantages of being small in back grinding amount, high in quality, energy-saving and environment-friendly.
The yield is as follows: considering the yield of the ratio of the actual production amount of the target product to the theoretical amount of the target product when the target product is completely produced, the yield is probably because the refinement is incomplete or byproducts are produced, namely the quotient of the quantity n of the produced mica powder and the total feeding quantity m is the yield c, and c is n/m
Comparative example:
a grinding method of high-quality synthetic mica comprises the following steps:
a. crushing: crushing mica into 200-2000 mu m mica sheets by ultrahigh pressure hydraulic power; the water pressure of the ultrahigh pressure water is 6-12 Mpa.
b. Separation: putting the mica slices into a centrifugal separator for solid-liquid separation, and spin-drying water;
c. grinding: selecting grinding equipment, adding grinding media or grinding aids, adding mica flakes, controlling moisture, grinding for 3-8 hours to form mica powder, pulping, and discharging; the grinding equipment is an edge runner mill, the rotating speed of the edge runner mill is 50-60HZ, the grinding aids are sodium hexametaphosphate accounting for 0.01-0.05% of the mass of the mica, sodium carbonate accounting for 0.01-0.05% of the mass of the mica and sodium hydroxide accounting for 0.01-0.03% of the mass of the mica, the grinding is carried out to control the water content to be 25-40%, and the water content is measured by a water content meter.
d. And (3) settling: and (3) pulping the ground mica powder, and separating the mica powder finished products of all the particle size sections by a hydraulic sedimentation method, wherein the solid-liquid ratio of classification by the hydraulic sedimentation method is 10-15%, and the hydraulic sedimentation method is a gravity sedimentation method, an ascending water flow method or a centrifugal sedimentation method.
The gravity settling method is that the particles and fluid are caused to move relatively to settle under the action of gravitational field, and the particles are concentrated in one direction under the action of gravitational field, or sink to the bottom of the container or float to the upper layer of the medium as long as the density of the particles and the medium is different.
An ascending water flow method: the typical apparatus of the ascending water flow method is a continuous decanter, and the basic principle is that the same ascending water quantity is utilized to generate different ascending water velocities in classifying pipes with different diameters, and ore particles with different particle sizes are divided into a plurality of particle sizes according to different settling velocities.
Centrifugal sedimentation method: the device used in the centrifugal sedimentation method is a series cyclone classifier, also called a cyclone water analyzer, and the basic principle is that the classification process is carried out in a centrifugal force field, and substances are thrown out at different heights according to different centrifugal forces to which the substances with different specific gravities are subjected.
The wheel mill is connected with an external power supply, a motor is started, 300 kg of mica flakes are slowly added, 100g of grinding aid sodium hexametaphosphate, 100g of sodium carbonate and 50g of sodium hydroxide are added, the grinding moisture is controlled to be 30-40%, the rotating speed of the mill is adjusted to 50HZ, grinding, discharging and grading are completed after 5 hours, and the yield of each particle size section is calculated.
The yield is as follows: considering the yield because the actual production amount of the target product is not completely refined or byproducts are generated, namely the quotient of the amount n of the generated mica powder and the total feeding amount m is the yield c, and c is n/m;
the yield of each particle size section after classification in examples and comparative examples;
Figure GDA0002997091150000071
the mica classified in the examples and comparative examples was surface-purified and activated, and then coated with a metal oxide.
Taking 10-60 μm as an example:
1. 40g of dry powder with the particle size of 10-60 mu m is put into a 1000ml beaker, purified water is added to 500ml, the mixture is stirred, the temperature is raised to 65-75 ℃, and the PH value is adjusted to 1.0-1.5.
2. 20ml of a 100g/L tin tetrachloride solution was uniformly added dropwise to the reaction vessel in step 1 over 1 hour. While the pH was kept constant by the addition of 32% sodium hydroxide. After the addition, the pH is adjusted to 2-3.
3. 150ml of 500g/L titanium tetrachloride solution was uniformly added dropwise to the reaction vessel in step 1 over a period of 10 hours. While the pH was kept constant by the addition of 32% sodium hydroxide. After stirring, washing, drying and calcining to obtain the pearlescent pigment with golden interference color.
Artificially synthesized fluorophlogopite powder with all particle size sections is produced according to the production method to obtain the pearlescent pigment with golden interference color, and the performance of the pearlescent pigment is detected by a coating or plate spraying method: taking a certain amount of pearlescent pigment produced by artificially synthesized mica powder of examples and comparative examples, adding a certain amount of resin, uniformly stirring, coating, and measuring the value by a color meter: see table below:
L a b c h
examples 30 to 100 μm 57.89 -0.09 28.44 28.44 90.19
Comparative examples 30 to 100 μm 55.7 1.06 27.57 27.59 87.8
Examples 10 to 60 μm 62.44 0.01 32.06 32.06 89.98
Comparative examples 10 to 60 μm 59.36 0.44 30.44 30.45 89.17
Examples 5 to 25 μm 60.07 1.56 31.27 31.31 87.15
Comparative examples 5 to 25 μm 57.12 1.52 26.57 26.61 86.73
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (1)

1. A grinding method of high-quality synthetic mica is characterized by comprising the following steps:
a. crushing: crushing mica into 200-2000 mu m mica sheets by ultrahigh pressure hydraulic power;
b. separation: putting the mica slices into a centrifugal separator for solid-liquid separation, and spin-drying water;
c. grinding: selecting grinding equipment, adding grinding media and grinding aids, adding mica flakes, controlling moisture, grinding for 3-8 hours to form mica powder, pulping, and discharging;
d. and (3) settling: pulping the ground mica powder, and separating the finished mica powder products of all particle size sections by a hydraulic sedimentation method;
the water pressure of the ultrahigh pressure water is 6-12 Mpa;
the grinding aid is sodium hexametaphosphate accounting for 0.01-0.05% of the mass of the mica, sodium carbonate accounting for 0.01-0.05% of the mass of the mica and sodium hydroxide accounting for 0.01-0.03% of the mass of the mica;
the grinding medium is zirconium beads/column with the specification of 10x10mm, 7.5x7.5mm and 5x5 mm;
the grinding equipment is a stirring mill, and the rotating speed of the stirring mill is 50-120;
the grinding control water content is 25% -40%, and the water content is measured by a water content measuring instrument;
the solid-liquid ratio of the classification by the hydraulic sedimentation method is 10-15 percent;
the hydraulic sedimentation method is a gravity sedimentation method, an ascending water flow method or a centrifugal sedimentation method.
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